WO2014041926A1 - Matériau actif d'électrode positive pour cellule secondaire au lithium-ion, électrode positive pour cellule secondaire au lithium-ion, et cellule secondaire au lithium-ion utilisant ceux-ci - Google Patents

Matériau actif d'électrode positive pour cellule secondaire au lithium-ion, électrode positive pour cellule secondaire au lithium-ion, et cellule secondaire au lithium-ion utilisant ceux-ci Download PDF

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Publication number
WO2014041926A1
WO2014041926A1 PCT/JP2013/071303 JP2013071303W WO2014041926A1 WO 2014041926 A1 WO2014041926 A1 WO 2014041926A1 JP 2013071303 W JP2013071303 W JP 2013071303W WO 2014041926 A1 WO2014041926 A1 WO 2014041926A1
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Prior art keywords
positive electrode
active material
electrode active
ion secondary
lithium
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PCT/JP2013/071303
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English (en)
Japanese (ja)
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小西　宏明
章 軍司
孝亮 馮
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株式会社日立製作所
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Priority to JP2014535447A priority Critical patent/JPWO2014041926A1/ja
Publication of WO2014041926A1 publication Critical patent/WO2014041926A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a positive electrode active material, a positive electrode, and a lithium ion secondary battery for a lithium ion secondary battery.
  • lithium ion secondary batteries have a higher energy density per weight than secondary batteries such as nickel metal hydride batteries and lead batteries, they are expected to be applied to electric vehicles and power storage systems. In order to meet the demand for electric vehicles, it is necessary to further increase the energy density, and it is necessary to increase the energy density of the positive electrode and the negative electrode.
  • a zLi [Li 1/3 M 2/3 ] O 2- (1-z) LiM′O 2 solid solution is expected.
  • M is one or more elements selected from Mn, Ti, and Zr
  • M ′ is one or more elements selected from Ni, Co, Mn, Fe, Ti, Zr, Al, Mg, Cr, and V. It is an element.
  • Patent Document 1 discloses that in a layered solid solution, x ⁇ Li [Li 1/3 Mn 2/3 ] O 2 ⁇ -y ⁇ LiNi 1/2 Mn 1/2 O 2 ⁇ -(1-xy) ⁇ LiCoO 2 ⁇ The composition with a large discharge capacity is examined along the ternary phase diagram.
  • Patent Document 1 since the discharge capacity shown in Patent Document 1 is a value when the discharge end potential is lowered to 2.0 V, a sufficient capacity can be obtained without discharging to a low potential of 2.0 V. It is not considered. Furthermore, the layered solid solution positive electrode generally has a drawback of high resistance at the end of discharge. Thus, at the end of discharge, there is a high possibility that a sufficient output cannot be obtained due to low potential and high resistance.
  • the present invention has been made in view of the above circumstances, and its object is to improve the increase in resistance at the end of discharge, which is a drawback of this material, and to increase the potential at the end of discharge.
  • a high-capacity positive electrode active material can be obtained, and a lithium ion secondary battery with reduced resistance increase at the end of discharge can be realized.
  • Composition formula zLi [Li 1/3 M 2/3 ] O 2- (1-z) LiM′O 2 (M is one or more elements selected from Mn, Ti, Zr, M ′ is Ni
  • the positive electrode active material represented by one or more elements selected from Co, Mn, Fe, Ti, Zr, Al, Mg, Cr, and V) is a conventional layered positive electrode active material LiMO 2 (M is a transition metal)
  • the positive electrode active material in the present embodiment solves such a problem.
  • the composition formula xLi 4/3 Mn 2/3 O 2 —yLiNi 1/2 Mn 1/2 O 2 — (1-x— y) LiMn 1-a M a O 2 (0 ⁇ x ⁇ 1,0 ⁇ y ⁇ 1, x + y ⁇ 1,0 ⁇ a ⁇ 0.02, M Al, Mg, Fe, Mo, W, V, Nb , Ti).
  • the positive electrode active material of the positive electrode material in the present embodiment will be described.
  • the positive electrode material in the present embodiment is mainly composed of Li, Ni, and Mn, and LiMnO 2 in which Mn is trivalent is dissolved in a positive electrode active material in which Mn is tetravalent.
  • the positive electrode active material in this embodiment does not contain Co, and has a higher potential at the end of discharge compared to a material containing Co, which is advantageous in terms of cost.
  • the material of this composition has a feature that the lithium diffusion resistance at the end of discharge is low, and the discharge potential does not rapidly decrease even at high rate discharge.
  • composition formula xLi 4/3 Mn 2/3 O 2 -yLiNi 1/2 Mn 1/2 O 2 - (1-x-y) LiMn 1-a M a O 2 (0 ⁇ x ⁇ 1,0 ⁇ y ⁇ 1, x + y ⁇ 1, 0 ⁇ a ⁇ 0.02, M Al, Mg, Fe, Mo, W, V, Nb, Ti) are used as positive electrode materials for lithium ion secondary batteries. When it is adopted, it is possible to achieve both resistance reduction at the end of discharge and low cost.
  • x, y values Li 4/3 Mn 2/3 O 2 and LiNi 1/2 Mn 1/2 O 2 and shows the percentage of the LiMn 1-a M a O 2 , 1 greater than 0 but less than ( 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1, x + y ⁇ 1).
  • x the capacity is approximately the same as that of the layered positive electrode, and a high capacity that is an advantage of the layered solid solution cannot be obtained.
  • This material is difficult to synthesize a single phase and easily generates impurities.
  • the crystal structure changes and the capacity decreases.
  • the values of x and y in the composition formula are 0.50 ⁇ x ⁇ 0.70 and x + y ⁇ 1.
  • the Li amount depends on x in the above relational expression and is 1.16 to 1.23, the Ni amount depends on y and is 0.1 to 0.225, and the Mn amount is 0.54 to 0.73.
  • the molar ratio of Mn is preferably larger than 0.61.
  • DCR direct current resistance
  • the conductivity in the positive electrode is improved with a material having higher electron conductivity than the lithium transition metal oxide.
  • Conductive paths are formed between lithium transition metal oxide particles by using particles that are coated with lithium transition metal oxide with a material having higher electron conductivity than lithium transition metal oxides, or by mixing a long conductive agent such as fibrous carbon. Form.
  • a conductive network between the positive electrode active material particles can be more easily formed by using fibrous carbon as a conductive material instead of spherical carbon as a conductive agent or together with carbon material particles.
  • a positive electrode for a lithium ion secondary battery is formed by forming a positive electrode mixture composed of a positive electrode active material, a conductive agent and a binder in a layered manner on a current collector.
  • a positive electrode mixture composed of a positive electrode active material, a conductive agent and a binder in a layered manner on a current collector.
  • an electrode in which fibrous carbon is highly dispersed is produced, and the conductivity of the electrode is improved.
  • It is also effective to construct a conductive network by coating the positive electrode active material with a material having high electron conductivity.
  • the positive electrode active material according to the present invention can be produced by a method generally used in the technical field to which the present invention belongs. For example, it can be prepared by mixing compounds containing Li, Ni, and Mn at an appropriate ratio and firing.
  • the composition of the positive electrode active material can be appropriately adjusted by changing the ratio of the compound to be mixed.
  • the compound containing Li include lithium acetate, lithium nitrate, lithium carbonate, and lithium hydroxide.
  • the compound containing Ni include nickel acetate, nickel nitrate, nickel carbonate, nickel sulfate, and nickel hydroxide.
  • Examples of the compound containing Mn include manganese acetate, manganese nitrate, manganese carbonate, manganese sulfate, manganese oxide, and the like.
  • the composition of the produced positive electrode active material can be determined by elemental analysis using, for example, inductively coupled plasma (ICP).
  • ICP inductively coupled plasma
  • a lithium ion secondary battery according to the present invention includes the above positive electrode active material.
  • a lithium ion secondary battery includes a positive electrode including a positive electrode active material, a negative electrode including a negative electrode active material, a separator, a conductive agent, a binder, an electrolytic solution, an electrolyte, and the like.
  • the negative electrode active material is not particularly limited as long as it is a material that can occlude and release lithium ions.
  • a material generally used in a lithium ion secondary battery can be used as the negative electrode active material.
  • graphite, a lithium alloy, etc. can be illustrated.
  • separator those commonly used in lithium ion secondary batteries can be used.
  • examples thereof include polyolefin microporous films and non-woven fabrics such as polypropylene, polyethylene, and a copolymer of propylene and ethylene.
  • conductive agent those generally used in lithium ion secondary batteries can be used. Examples thereof include acetylene black and ketjen black.
  • binder those generally used in lithium ion secondary batteries can be used.
  • binder those generally used in lithium ion secondary batteries can be used.
  • polyvinylidene fluoride, an imide binder, an acrylic binder and the like can be exemplified.
  • electrolytic solution and the electrolyte those generally used in lithium ion secondary batteries can be used.
  • diethyl carbonate, dimethyl carbonate, ethylene carbonate, propylene carbonate, vinylene carbonate, methyl acetate, ethyl methyl carbonate, methyl propyl carbonate, dimethoxyethane and the like can be exemplified as the electrolytic solution.
  • FIG. 1 is a cross-sectional view of an essential part schematically showing the structure of a lithium ion secondary battery in the present embodiment.
  • a lithium ion secondary battery 10 shown in FIG. 1 includes an electrode having a positive electrode plate 1 coated with a positive electrode material on both sides of a current collector, a negative electrode plate 2 coated with a negative electrode material on both sides of the current collector, and a separator 3. Provide a group.
  • the positive electrode plate 1 and the negative electrode plate 2 are wound through a separator 3 to form a wound electrode group. This wound body is inserted into the battery can 7.
  • the negative electrode plate 2 is electrically connected to the battery can 7 through the negative electrode lead piece 5.
  • a sealing lid 6 is attached to the battery can 9 via a packing 8.
  • the positive electrode plate 1 is electrically connected to the sealing lid portion 6 via the positive electrode lead piece 4.
  • the wound body is insulated by the insulating plate 9.
  • the electrode group may not be a wound body as shown in FIG. 1, but may be a laminated body in which the positive electrode plate 1 and the negative electrode plate 2 are laminated via the separator 3.
  • Lithium acetate, nickel acetate, and manganese acetate were dissolved in purified water, and then spray dried using a spray drying apparatus to obtain a precursor.
  • the obtained precursor was calcined in the atmosphere at 500 ° C. for 12 hours to obtain a lithium transition metal oxide.
  • the obtained lithium transition metal oxide was pelletized and then fired at 850 to 1050 ° C. for 12 hours in the air.
  • the fired pellets were pulverized in an agate mortar and classified with a 45 ⁇ m sieve to obtain a positive electrode active material.
  • Table 1 shows the composition of the prepared positive electrode active material and the positive electrode active materials used in the respective examples and comparative examples.
  • the compositions shown in Table 1 are values determined by composition analysis such as ICP.
  • a positive electrode active material, a conductive agent, and a binder are uniformly mixed to produce a positive electrode slurry (positive electrode material). Then, the positive electrode slurry is applied onto an aluminum current collector foil having a thickness of 20 ⁇ m, dried at 120 ° C., and compression-molded so as to have an electrode density of 2.2 g / cm 3 by pressing to obtain an electrode plate. It was. Thereafter, the electrode plate was punched into a disk shape having a diameter of 15 mm to produce a positive electrode.
  • the negative electrode was produced using metallic lithium.
  • 1.0 mol / liter LiPF 6 was dissolved in a mixed solvent of EC (ethylene carbonate) and DMC (dimethyl carbonate) at a volume ratio of 1: 2.
  • the prototype battery was subjected to a charge / discharge test with a current equivalent to 0.05 C, an upper limit voltage of 4.8 V, a discharge equivalent to 1 C, and a lower limit voltage of 2.5 V.
  • the discharge capacity ratio was improved as compared with Comparative Example 1. This is considered to be because the composition of the positive electrode active material is in the range of 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1, and x + y ⁇ 1.
  • the discharge capacity ratio was a high value. This is because the composition ratio of xLi 4/3 Mn 2/3 O 2 —yLiNi 1/2 Mn 1/2 O 2 — (1-xy) LiMnO 2 is 0.50 ⁇ x ⁇ 0.70. This is probably because 2 ⁇ y ⁇ 0.45 and 0.8 ⁇ x + y ⁇ 0.95.
  • the molar ratio of Ni is preferably less than 30% with respect to the total amount of Ni and Mn.
  • Comparative Example 6 it is composed only of LiNi 1/2 Mn 1/2 O 2 and does not contain Li 4/3 Mn 2/3 O 2 or LiMnO 2 , so that the layered positive electrode and capacity are The high capacity that is the advantage of the layered solid solution cannot be obtained.
  • FIG. 2 shows the composition range of the positive electrode active material used in Examples 1 to 6.
  • 2 in FIG. 2 shows the entire ternary phase diagram, and the inside of the frame 12 shows the composition range of Examples 1 to 6 having particularly excellent characteristics.
  • this composition range a material having a low resistance increase at the end of discharge can be obtained.
  • the positive electrode produced by applying the positive electrode material shown in the present embodiment as the positive electrode plate 1 of the lithium ion secondary battery 10 the high capacity and high safety lithium ion secondary battery 10 can be obtained. Obtainable. Therefore, according to this invention, the positive electrode material which can achieve the high energy density requested
  • the present invention can be used for a positive electrode material of a lithium ion secondary battery and a lithium ion secondary battery, and in particular, can be used for a lithium ion secondary battery for an electric vehicle.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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Abstract

Selon la présente invention, une cellule secondaire au lithium-ion ayant une augmentation minimale de résistance à la fin d'une décharge est obtenue par utilisation d'un matériau actif d'électrode positive représenté par la formule de composition suivante. Formule de composition : xLi4/3Mn2/3O2-yLiNi1/2Mn1/2O2-(1-x-y)LiMN1-aMaO2 (0 < x < 1, 0 < y < 1, x+y < 1, 0 ≤ a ≤ 0,02, M = Al, Mg, Fe, Mo, W, V, Nb, Ti)
PCT/JP2013/071303 2012-09-12 2013-08-07 Matériau actif d'électrode positive pour cellule secondaire au lithium-ion, électrode positive pour cellule secondaire au lithium-ion, et cellule secondaire au lithium-ion utilisant ceux-ci WO2014041926A1 (fr)

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JP2014535447A JPWO2014041926A1 (ja) 2012-09-12 2013-08-07 リチウムイオン二次電池用正極活物質、リチウムイオン二次電池用正極材料、リチウムイオン二次電池用正極、およびそれを用いたリチウムイオン二次電池

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JP2012-200066 2012-09-12
JP2012200066 2012-09-12

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006253119A (ja) * 2005-02-08 2006-09-21 Mitsubishi Chemicals Corp リチウム二次電池正極材料用リチウムニッケルマンガンコバルト系複合酸化物粉体及びその製造方法、並びにそれを用いたリチウム二次電池用正極及びリチウム二次電池
JP2011154997A (ja) * 2009-12-29 2011-08-11 Gs Yuasa Corp リチウム二次電池用活物質、リチウム二次電池用電極、リチウム二次電池及びその製造方法
JP2012022888A (ja) * 2010-07-14 2012-02-02 Hitachi Ltd 非水電解質二次電池及びそれを有する電池システム

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5625273B2 (ja) * 2009-07-24 2014-11-19 日産自動車株式会社 リチウムイオン電池用正極材料の製造方法
JP5700274B2 (ja) * 2009-08-21 2015-04-15 株式会社Ｇｓユアサ リチウム二次電池用活物質、リチウム二次電池用電極、リチウム二次電池及びその製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006253119A (ja) * 2005-02-08 2006-09-21 Mitsubishi Chemicals Corp リチウム二次電池正極材料用リチウムニッケルマンガンコバルト系複合酸化物粉体及びその製造方法、並びにそれを用いたリチウム二次電池用正極及びリチウム二次電池
JP2011154997A (ja) * 2009-12-29 2011-08-11 Gs Yuasa Corp リチウム二次電池用活物質、リチウム二次電池用電極、リチウム二次電池及びその製造方法
JP2012022888A (ja) * 2010-07-14 2012-02-02 Hitachi Ltd 非水電解質二次電池及びそれを有する電池システム

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